US8202347B2 - Process for recycling aluminum alloy scrap coming from the aeronautical industry - Google Patents

Process for recycling aluminum alloy scrap coming from the aeronautical industry Download PDF

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US8202347B2
US8202347B2 US12/304,548 US30454807A US8202347B2 US 8202347 B2 US8202347 B2 US 8202347B2 US 30454807 A US30454807 A US 30454807A US 8202347 B2 US8202347 B2 US 8202347B2
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scrap
molten metal
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US20090285716A1 (en
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Jean-Francois Verdier
Jean-Remi Butruille
Michel Leroy
Didier Valax
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Constellium Issoire SAS
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Constellium France SAS
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/005—Preliminary treatment of scrap
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B21/00—Obtaining aluminium
    • C22B21/06—Obtaining aluminium refining
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the invention relates to the manufacture of aluminum alloy remelt ingots from scrap (raw materials for recycling, such as chips or machining off-cuts).
  • the invention particularly relates to the recycling of scrap resulting from the manufacturing processes of the aircraft and space industries.
  • Patent applications JP07166259, JP07207378, JP09178149 and JP09263853 seek to solve the problem of recycling plated sheets designed for the manufacture of heat exchangers by brazing.
  • the scrap from these products contains several percent of silicon by weight, which makes recycling difficult.
  • Processes including a fractional, crystallization stage and a final stage involving pressing the crystals formed to eject the residual liquid are described in these patent applications. These processes aim to eliminate the silicon.
  • the special problems posed by the purification of iron are not dealt with in these requests.
  • Patent EP 1 101 830 (Pechiney Rhenalu) describes a manufacturing process for an intermediate product in a given alloy of series 7XXX from recycling products. In order to be able to recycle off-cuts from different alloys of the 7XXX series without having to carry out sorting, this patent describes a process including at least one refining stage of said recycling products making it possible to reduce the content of a peritectic element such as Cr or Zr with the help, for example, of a selective precipitating agent including boron.
  • the applicant therefore sought a manufacturing process for intermediate products using scrap from the aircraft industry which would facilitate recycling of series 7XXX and series 2XXX alloys.
  • a first subject of the invention is a manufacturing process for a remelt block containing aluminum designed for making aluminum alloy for the aircraft industry in which
  • a second subject of the invention is a remelt block obtained by the process according to the invention characterized in that its average iron content is 5 times lower than that of the initial molten metal bath obtained at the conclusion of the smelting stage.
  • Yet another subject of the invention is a manufacturing process for a semi-finished product in which at least one remelt block obtained by the process according to the invention is melted.
  • Yet another subject of the invention is the use of a semi-finished product obtained by the process according to the invention for the manufacture of an aircraft structural element.
  • FIG. 1 illustrates a segregation device which can be used in the context of the invention.
  • FIG. 2 illustrates the change in temperature of the molten metal according to the crystallization time for the various tests carried out.
  • FIG. 3 illustrates the change in purification rate as a function of the speed of crystallization programmed.
  • machining includes any process for removing matter such as turning, milling, drilling, boring, tapping, electroerosion, resurfacing and polishing.
  • the term “semi-finished product” is used to mean a semi-finished product designed to be worked as, in particular, a plate for rolling, an ingot for extruding, a block for forging.
  • the term “remelt block” indicates a semi-finished product intended to be remelted, containing aluminum and for which the sum of the Zn, Cu, Mg and Li contents is at least 3% by weight.
  • the sum of the Zn, Cu, Mg and Li contents is at least 4% by weight and in a preferred method at least 5% by weight, in the remelt blocks according to the invention.
  • structural element refers to a part used in mechanical engineering for which the mechanical, static and/or dynamic characteristics are of particular importance for the performance and the integrity of the structure, and for which a structural analysis is generally prescribed or carried out.
  • these structural elements include the parts which make up the fuselage (such as the fuselage skin, stringers, bulkheads, circumferential frames), the wings (such as the wing skin, stringers or stiffeners, ribs and spars) and the tail unit, made up of horizontal and vertical stabilizers, as well as floor beams, seat tracks and doors.
  • the process according to the invention includes the stages of: supplying the scrap, smelting it, purifying it by segregation, recovering the solidified mass, optionally purifying the peritectic elements and manufacturing the semi-finished products.
  • the various stages of the process according to the invention can be implemented continuously, semi-continuously or discontinuously (batch). It is possible in certain embodiments to carry out certain stages continuously, such as for example the smelting stage, and other stages discontinuously, such as for example the segregation stage.
  • certain stages continuously such as for example the smelting stage
  • other stages discontinuously such as for example the segregation stage.
  • the various stages quoted in the preceding paragraph are carried out successively.
  • Scrap suitable for being recycled by the process according the present invention may take various forms.
  • scrap is in massive form it is generally used for direct smelting.
  • scrap is in divided form, such as chips, turnings, off-cuts or clippings and covered with lubricants which may be whole emulsions or oils and which are referred to here by the general term “oils”.
  • the amount of oil present on scrap varies according to the manufacturing stage during which it is generated and the technology used for removing the metal.
  • the amount of oil present on the scrap obtained during the scalping operation for rolling plates is generally small, but the amount of oil present on scrap from machining operations is much greater. No matter how much oil is on the scrap, the present invention can be used.
  • a preliminary de-oiling stage may possibly prove to be necessary or at least useful. It can be carried out using any conventional chemical and/or heat cleaning methods.
  • An advantageous degreasing method involves using a cylindrical, revolving furnace with burner (IDEX® type); the atmosphere of this type of furnace contains little oxygen, typically less than 5% or even 1%, to prevent the oils from igniting.
  • the oxygen content is managed in this type of furnace using a measurement probe and a control loop.
  • Compacted scrap may require a crushing stage.
  • the scrap used in the context of this invention contains mainly aluminum alloys used in the aircraft industry, i.e. it comprises at least 50%, preferably at least 70% and even more preferably at least 90% of aluminum alloys used in the aircraft industry.
  • aluminum alloys used in the aircraft industry means alloys belonging to series 2XXX, 6XXX and 7XXX. It is preferable that the scrap used in the context of this invention be sorted so that it comprises mainly series 7XXX alloys or series 2XXX alloys, i.e. the scrap comprises at least 50%, preferably at least 70%, and even more preferably at least 90% of alloys from the selected series.
  • these alloys are suitably sorted, i.e.
  • scrap from a different series from that of the scrap to be recycled is preferably limited to 5% and, even more advantageously, to 1%.
  • Suitable series 7XXX alloys are in particular alloys 7010, 7040, 7050, 7150, 7250, 7055, 7056, 7068, 7049, 7140, 7149, 7249, 7349, 7449, 7075, 7175 and 7475.
  • For series 2XXX alloys it is advantageous to separate alloys containing lithium and/or silver from alloys that do not contain any in amounts above impurity level, typically 0.05% by weight.
  • Suitable series 2XXX alloys that do not contain lithium and/or silver are in particular alloys 2014, 2022, 2023, 2024, 2026, 2027, 2056, 2224, 2324 and 2524.
  • Suitable series 2XXX alloys that do contain lithium and/or silver are in particular alloys 2050, 2090, 2091, 2094, 2095, 2097, 2098, 2099, 2039, 2139, 2195, 2196, 2197, 2199, 2297 and 2397, as defined by Aluminum Association.
  • the advantage of using sorted waste is to facilitate the use of remelt blocks obtained by the process according to the invention in alloys of the same series.
  • the process according to the invention is also advantageous for recycling scrap containing scandium.
  • the scrap used in the context of this invention should not be polluted with Fe and Si by waste that is not aluminum alloy.
  • the process according to the invention may include a stage for reducing the amount of ferrous waste.
  • Ferrous metals can be separated out by magnetic and/or eddy current sorting; this latter method being particularly appropriate for separating magnetic waste (white metals, stainless steel, etc.) and non-magnetic (red metals, copper, brass, etc.).
  • the Fe content of scrap from ferrous alloy parts can in this way be limited.
  • Scrap sorting can be improved still further by using a device based on the differences in particle size, density and/or electrical conductivity as described in U.S. Pat. No. 5,060,871.
  • the supply stage may include, depending on the initial definition of scrap, the operations of:
  • Scrap is smelted in a smelting furnace to give an initial molten metal bath.
  • the scrap used contains mainly aluminum alloys used in the aircraft industry, the sum of the Zn, Cu, Mg and Li contents in the initial molten metal bath is always greater than 4% by weight.
  • the sum of the Zn, Cu, Mg and Li contents is greater than 6% by weight and in a preferred method greater than 8% by weight, in the initial molten metal bath.
  • the smelter used is a furnace with electromagnetic agitation (an induction furnace), as this type of furnace makes it possible to limit the combustion of scrap.
  • an induction furnace an induction furnace
  • the main aluminum purification processes known are the electrolysis purification process (known as a “three-layer process” or “Gadeau process”) and the purification process by fractional crystallization (known as a “segregation” process). These processes are used in the aluminum industry solely to obtain metal of very high purity (typically with an aluminum content greater than 99.9% by weight and as much as 99.999%) from metal that is already relatively pure (typically with an aluminum content greater than 99.5% by weight, or even greater than 99% by weight). So patents EP 0 091 386 and U.S. Pat. No. 6,406,515 (Aluminum Pechiney) or U.S. Pat. No.
  • 4,734,127 (Nipponese Light Metal) describe processes for the segregation of liquid aluminum with a total content of impurities of around 500 to 1500 ppm (or an aluminum content higher than 99.85% by weight) and do not consider applying these processes for starting metals with aluminum contents of less than 99% by weight.
  • the segregation process makes it possible to purify elements with a low partition coefficient.
  • the partition coefficient is the ratio between the balance between the concentration of the element in the solid phase and its concentration in the liquid phase.
  • the freezing range i.e. the variation in temperature between the liquidus and the solidus of charged alloys is much greater than that of pure metal.
  • the temperature of the molten metal changes much more with the degree of purification in the case of a charged alloy than for a pure metal.
  • the residual liquid which takes on impurities during purification may reach the eutectic point at which precipitation of intermetallic particles occurs. These intermetallic particles are likely to mix with the purified crystals, thereby greatly reducing purification.
  • the number of elements interacting in a charged alloy makes it difficult or even impossible to make theoretical forecasts as to the outcome of the purification. So the partition coefficient, which is known fairly accurately for binary mixtures, is unknown in the case of a charged alloy such as a 2XXX or 7XXX alloy.
  • fractional crystallization processes in which the metal is solidified on a cooled rotor may be used.
  • Fractional crystallization processes can also be implemented, in which a furnace with a cooled bottom is used, as described for example in patent application JP 58-104132.
  • Patent FR 2 788 283 (Aluminium Pechiney) also describes a process including partial remelting to obtain refined and ultra-refined metal while periodically, and in a controlled way, tamping down crystals formed by fractional crystallization.
  • This patent also describes a device making it possible to use said process.
  • the solidified mass undergoes at least partial remelting during the segregation stage to increase the purification coefficient
  • FIG. 1 illustrates a device which can be used advantageously within the context of the invention for the segregation phase.
  • the device includes a heat-resistant crucible ( 4 ), a furnace ( 6 ) provided with at least one means of heating ( 5 ), at least one means of tamping ( 1 ), including a tamping end-piece ( 12 ), a stem interdependent of this end-piece ( 11 ) and means for moving the stem-end unit ( 13 ) vertically.
  • Molten scrap ( 2 ) is contained in the heat-resistant crucible ( 4 ) and crystallization giving a solidified mass ( 3 ) is obtained through a drop in temperature of the molten metal.
  • the device includes a means to measure the height of the solid mass H and means such as a control unit ( 21 ) and a power unit ( 22 ) to control the means of heating according to the height of the solid mass H measured and the target value H′ in order to obtain a predetermined crystallization speed.
  • the means of tamping ( 1 ) makes it possible both to tamp down the crystals formed and to measure the height H of the solid mass.
  • the tamping means is alternately immersed and emersed, the time between two successive emersions being between 20 seconds and 10 minutes.
  • the crystallization speed given as the mass of crystals formed, expressed as a percentage of the weight initially charged, per hour of crystallization is between about 3.8%/h and about 6.2%/h, and preferably ranging between 4%/h and 6%/h.
  • the crystallization speed is preferably between about 90 kg/h (kilograms per hour) and about 140 kg/h and in a preferred method between about 100 kg/h and about 130 kg/h.
  • the crystallization speed is too high, purification is poor and a solid mass is obtained with a composition close to that of molten scrap. In this case, the partial remelting of the crystals formed during the operation, which is a very favorable factor for the purification, is too limited. If the crystallization speed is too low, intermetallic particles may become incorporated into the solidified mass and reduce its purity. In addition, if the crystallization speed is too low, the operation is likely to lose its economic worth.
  • the “yield” of the segregation stage is the relationship between the mass of the remelt block obtained and the initial mass of scrap melted. This yield can be expressed as a percentage. If the yield is too low, the segregation stage is of no economic value. If the yield is too high, the residual liquid at the end of the stage is highly charged with alloy elements that can cause the formation of intermetallic particles detrimental to the purity of the solidified mass and also make this impure residual liquid difficult to develop economically.
  • the yield of the segregation stage is between about 50% and about 90% and preferably between about 60% and about 80%.
  • fractional crystallization is carried out using a device including a heat-resistant crucible ( 4 ), a furnace ( 6 ) provided with at least one means of heating ( 5 ), at least one means of tamping ( 1 ), including a tamping end-piece ( 12 ), a stem interdependent of this end-piece ( 11 ) and a means for moving the stem/end-piece unit ( 13 ) vertically, a means of measurement for continuously measuring the temperature of the molten metal and a control loop to control the means of heating as a function of the temperature of the molten metal.
  • a predetermined reduction curve is imposed on the temperature of the molten metal.
  • the reduction in the temperature of the molten metal is between 1 and 5° C./h and preferably between 2 and 4° C./h.
  • the segregation stage is stopped according to the temperature of the molten metal.
  • the segregation stage is stopped when the temperature of the molten metal reaches 570° C. and preferably when it reaches 580° C.
  • the residual liquid is separated from the solidified mass.
  • this separation is carried out by draining, by tipping the heat-resistant crucible in which the segregation stage was carried out.
  • the tipping angle is chosen in order to quickly drain the liquid without running the risk of allowing the solidified mass to drop.
  • the residual liquid is sucked up using appropriate means.
  • the solidified mass is recovered using appropriate means. If the solidified mass is in a heat-resistant crucible, the surface of the mass can advantageously be broken in order to introduce a means of lifting making it possible to extract the solidified mass from the heat-resistant crucible.
  • the solidified mass obtained can be used as a remelt block either as it is, or machined on its surface and/or sawn to be used as a remelt block.
  • the remelt block according to the invention is characterized in that its average iron content is 5 times lower and preferably 10 times lower than that of the initial molten metal bath obtained at the conclusion of the smelting stage.
  • the iron content and silicon content of the remelt block according to the invention are less than 0.1% by weight and preferably lower than 0.05% by weight.
  • the weight of the remelt blocks according to the invention is at least 1000 kg and preferably at least 1300 kg.
  • this stage may be advantageous to carry out an additional stage which involves purifying the peritectic elements, i.e. the elements whose partition coefficient is greater than 1, and in particular chromium and zirconium.
  • this stage is carried out by precipitating at least one peritectic element using a selective precipitating agent including boron, and separating the precipitation products formed.
  • the remelt blocks obtained by the process according to the invention can be used for the manufacture of semi-finished products designed for the aircraft industry.
  • the remelt blocks according to the invention are advantageous because they provide alloy elements such as Zn Cu, Mg and Li without bringing in impurities such as Fe and Si, which would not be possible by adding scrap containing mainly aluminum alloys used in the aircraft industry directly.
  • At least one remelt block according to the invention is melted, possibly with of other types of aluminum ingots, an alloy designed for the aircraft industry is made, typically an alloy of series 7XXX or series 2XXX, and this alloy is cast in the shape of a semi-finished product.
  • the semi-finished product obtained can be used to manufacture a structural element of an aircraft.
  • FIG. 1 illustrates the device used for the tests.
  • the means of tamping makes it possible to measure the height H of crystals formed.
  • a control loop acting on the heating power level is used to program the crystallization speed to a predetermined value.
  • FIG. 2 shows how temperature changes with crystallization speed.
  • the residual molten metal was analyzed at the end of the operation.
  • the residual molten metal was drained at the end of the test by tipping the crucible. This final operation could not be performed for test 4.
  • Solidified metal was finally extracted from the crucible and weighed.
  • a purification indicator X i is calculated for each element i as follows:
  • FIG. 3 illustrates the results obtained.
  • the best results in terms of purification of iron are obtained for tests 3 and 4. No significant increase in the purification of the elements Cu, Mg and Zn for these tests is to be observed, which therefore represent a particularly favorable compromise.
  • the poorer performance obtained for tests 1 and 2 might be related to the intermetallic crystal precipitation of type Al 3 Fe.
  • the temperature reached by the molten metal at the end of these tests (see FIG. 2 ) is close to the temperature estimated using models for the start of precipitation).
  • test conditions 1, 2, 5 or 6 may prove to be sufficient, in particular for mixtures of scrap only slightly enriched in iron and silicon which do not require thorough purification.

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US12/304,548 2006-06-23 2007-06-18 Process for recycling aluminum alloy scrap coming from the aeronautical industry Active 2029-04-14 US8202347B2 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR0605642 2006-06-23
FR0605642A FR2902800B1 (fr) 2006-06-23 2006-06-23 Procede de recyclage de scrap en alliage d'aluminium provenant de l'industrie aeronautique
PCT/FR2007/001005 WO2007147962A2 (fr) 2006-06-23 2007-06-18 Procede de recyclage de scrap en alliage d'aluminium provenant de l'industrie aeronautique

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US20090285716A1 US20090285716A1 (en) 2009-11-19
US8202347B2 true US8202347B2 (en) 2012-06-19

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US (1) US8202347B2 (ru)
EP (1) EP2038440B1 (ru)
JP (2) JP5620099B2 (ru)
CN (1) CN101473053B (ru)
CA (1) CA2654159C (ru)
ES (1) ES2397477T3 (ru)
FR (1) FR2902800B1 (ru)
RU (1) RU2441926C2 (ru)
WO (1) WO2007147962A2 (ru)

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RU2009102055A (ru) 2010-07-27
CN101473053A (zh) 2009-07-01
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FR2902800A1 (fr) 2007-12-28
JP5620099B2 (ja) 2014-11-05
EP2038440B1 (fr) 2012-10-17
US20090285716A1 (en) 2009-11-19
EP2038440A2 (fr) 2009-03-25
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CA2654159A1 (fr) 2007-12-27
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